CN104556674B - A kind of preparation method of rare earth ion co-doped fiber prefabricated rods - Google Patents
A kind of preparation method of rare earth ion co-doped fiber prefabricated rods Download PDFInfo
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- CN104556674B CN104556674B CN201510055355.5A CN201510055355A CN104556674B CN 104556674 B CN104556674 B CN 104556674B CN 201510055355 A CN201510055355 A CN 201510055355A CN 104556674 B CN104556674 B CN 104556674B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
- C03B37/018—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
- C03B37/01807—Reactant delivery systems, e.g. reactant deposition burners
- C03B37/01838—Reactant delivery systems, e.g. reactant deposition burners for delivering and depositing additional reactants as liquids or solutions, e.g. for solution doping of the deposited glass
Abstract
The present invention relates to a kind of preparation method of rare earth ion co-doped fiber prefabricated rods.Prepare multiple rare earth ions respectively and aluminium ion is co-doped with the aqueous solution of agent；Select quartzy base tube and access MCVD lathe, after high temperature polishing, be sequentially depositing sealing coat and porous core layer；Hollow barred body containing porous core layer is fixed on lowering or hoisting gear, barred body is partially soaked in solution；Ratio and concentration are co-doped with to what ion was co-doped with that ratio distribution and concentration distribution change various ions in solution according to the excellent mandrel being pre-designed, pass through the lowering or hoisting gear regulation length soaked in the solution of barred body simultaneously；Soaked barred body is accessed MCVD lathe again, after drying and dehydrating, barred body collapsing is finally become solid bar by porous core layer vitrification.The ion that this method can flexibly accurately control in prefabricated rods core axial direction is co-doped with the distribution of ratio and doping content, finds optimal ion for variety classes rare earth ion co-doped fiber and is co-doped with ratio and a kind of doping content highly effective short-cut method of offer.
Description
Technical field
The present invention relates to optic fibre manufacture process, more particularly, to a kind of preparation method of rare earth ion co-doped fiber prefabricated rods.
Background technology
1985, the research worker of Southampton, Britain university adopted modified chemical vapor deposition technique (Modified
Chemical Vapour Deposition, MCVD) successfully develop rare earth doped fiber.In the last thirty years, research worker is continuous
Ground improves to the preparation technology of rare earth doped fiber and innovates, and then Rare-earth Doped OFAs and laser instrument are obtained
Continue, quickly develop.Laser instrument and application technology are important optoelectronic areas forward position skills being related to national defence, the people's livelihood
Art, the light compared with laser instrument other types of with semiconductor laser, gas laser etc., with rare earth doped fiber as gain media
Fibre laser has the advantages that high light beam quality, high efficiency, Low threshold, tunable, narrow linewidth and high performance-price ratio, and mixes rare earth light
Fibre is the critical material that restriction fiber amplifier and laser instrument develop further, and therefore, we must improve further and mix rare earth
The performance of optical fiber, the rare earth doped fiber of developing new product variety.
For constantly lifting the performance of fiber amplifier and laser instrument, research worker is mixing the basis of single rare earth element optical fiber
On, develop rare earth ion co-doped fiber, at present, the rare earth ion co-doped fiber making progress larger is mainly erbium and ytterbium codoping light
Fibre, the rare earth ion co-doped fiber of other species is still in theoretical and exploratory stage.Below, to dilute taking erbium-ytterbium co-doped fiber as a example
The performance of native ion co-doped fiber and advantage illustrate：Compared with Er-doped fiber, erbium-ytterbium co-doped fiber mainly has the advantage that：
Yb3+There is absorption band (800 ~ 1070nm) and the excitation band of non-constant width, greatly extend the scope of pump light source；Yb3+No dense
Degree quenching phenomenon, can be with high-concentration dopant；Yb3+Absorption cross-section be much larger than Er3+, it is easier to absorb the pumping luminous energy near 980nm
Amount；Yb3+'s2F5/2Can band and Er3+'s4I11/2Can band be closer to, ion energy is very easy to from Yb3+'s2F5/2Can band transfer
To Er3+'s4I11/2On carrying, then radiationless transition is arrived4I13/2Can carry, finally give off photon, return to4I15/2Can band.However,
For fiber amplifier and laser instrument, Er3+、Yb3+Concentration when reaching certain optimal proportion, the performance of system can be only achieved
Good.If Er3+Doping content is too high, can lead to Er3+Occur to assemble and Energy upconversion phenomenon；If Yb3+Excessive concentration, then
Lead to Yb3+Energy conversion ion each other occurs so that the absorption efficiency of pump power reduces.Especially when needing high concentration
Doping Er3+And Yb3+When, the good Er of more GPRS3+、Yb3+It is co-doped with ratio with aluminum, phosphorus etc. are co-doped with ion.For high concentration rare earth from
Sub- co-doped fiber, for finding the ratio that is most preferably co-doped with, if using traditional solution doping technique, needing to carry out lot of experiments, system
Standby substantial amounts of prefabricated rods, so both take a significant amount of time, and are unfavorable for saving R＆D costs again.Therefore, for high concentration rare earth from
The development of sub- co-doped fiber is it is necessary to develop a kind of efficient preparation method.
High-capacity optical fiber laser cannot be only used for the technical fields such as industry cutting, welding it can also be used to national defense and military is led
Domain, high-capacity optical fiber laser can be used for attacking enemy's battlebus, naval vessel, guided missile, or even in-orbit airship, satellite etc..However, mixing dilute
Heat effect in native optical fiber seriously governs the lifting further of laser power.Improve the profit of rare earth doped fiber Rare Earth Ion
It is to reduce a kind of important effective means of optical fiber heat effect with rate, in high-concentration dopant optical fiber, near the rare earth at pumping end
Ion can sponge more pump energy, more remote apart from pumping end, and remaining pump energy is fewer, therefore, far-end dilute
Native ionic availability is relatively low, ion can be led to occur energy to change each other, and then produce unnecessary heat effect.For with
Upper problem, research worker proposes the concept of grade doping, and that is, from the beginning of pumping end, the doping gradually reducing rare earth ion is dense
Degree, and then improve the utilization rate of rare earth ion.However, there is presently no effective technological means preparation gradient rare earth doped fiber.
Content of the invention
The purpose of the present invention is the deficiency for existing rare earth doped fiber preparation method, provides a kind of rare earth ion to be co-doped with light
The preparation method of fine prefabricated rods, the method is passed through to control and is soaked various in the height and position of prefabricated rods and solution in the solution being co-doped with
The change of ion concentration, reaches the effect controlling the upper various ion doping concentration distributions of rare earth doped fiber axial direction.
The present invention is completed by technical scheme below：A kind of preparation method of rare earth ion co-doped fiber prefabricated rods, its feature
It is, the preparation of rare earth ion co-doped fiber prefabricated rods adopts MCVD technique and solution doping technique, and the method includes following preparation
Step：
（1）. prepare multiple rare earth ions respectively and aluminium ion is co-doped with the aqueous solution of agent；
（2）. select quartzy base tube and access MCVD lathe, after high temperature polishing, be sequentially depositing sealing coat and porous core layer；
（3）. the hollow barred body containing weaker zone is fixed on electrical-controlled lifting device, initial period is it is ensured that contain loose
The barred body part of sandwich layer is completely soaked in the solution；
（4）. according to the excellent mandrel being pre-designed to ion be co-doped with ratio distribution and concentration distribution, change solution in various from
The length being co-doped with ratio and concentration, passing through that electrical-controlled lifting device regulation barred body soaks in the solution simultaneously of son；
（5）. soaked barred body is accessed MCVD lathe again, after drying and dehydrating, porous core layer vitrification finally will
Hollow barred body collapsing becomes solid bar.
It is an advantage of the invention that：Can flexibly accurately control the ion in prefabricated rods core axial direction be co-doped with ratio with adulterate dense
The distribution of degree, finds optimal ion for variety classes rare earth ion co-doped fiber and is co-doped with ratio and doping content offer a kind of ten
Divide effective short-cut method, scientific research efficiency can be lifted, also can reduce R＆D costs simultaneously.Additionally, it is suitable for gradient
The preparation of rare earth ion doped optical fiber prefabricated rod.
Brief description
Fig. 1 is the structural representation of rare earth ion liquid phase doping device；
The prefabricated rods cross-sectional view that Fig. 2 is prepared for the present invention.
Specific embodiment
Below in conjunction with drawings and Examples, the invention will be further described：
This method is adopted to prepare the excellent core segment of preform with silicon dioxide as substrate, except at least two rare earths that adulterate
Outside ion, in plug, also can mix the elements such as aluminum and phosphorus simultaneously.Excellent mandrel ion upwards is co-doped with ratio with doping content at least
One is had to be different.Rare earth ion by solution doping technique mix prefabricated rods, made by way of solution soaking rare earth from
Son is immersed in the loose shape sandwich layer hole of prefabricated rods.If needing in sandwich layer to mix aluminium element, aluminium ion passes through solute doping
Method mixes；If needing in sandwich layer to mix P elements, P elements are mixed by gas phase doping method.Barred body containing porous core layer hangs down
Directly put into equipped with the container of rare-earth ion solution, in immersion process, barred body can be adjusted by electrical-controlled lifting device
Highly, initial period it is ensured that the barred body part containing porous core layer is completely soaked in the solution, that is, controls barred body to soak in the solution
The length of bubble.During prefabricated rods are constantly lifted, by constantly injection rare-earth ion solution or constantly note in a reservoir
The mode entering deionized water changes original solution concentration or the ratio of rare earth ion concentration.When the continuous ion changing in solution
When concentration and ion are co-doped with ratio, it is different that excellent core exceeds the part of liquid level and the impact that the part less than liquid level is subject to, and enters
And make excellent core have different ions in the axial direction and be co-doped with ratio and doping content.
The introducing of impurity should be avoided in solution process for preparation, and the raw material of higher degree should be selected as far as possible；Step（1）In,
The aqueous solution that rare earth ion, aluminium ion are co-doped with agent adopts rare earth chloride, aluminum chloride and alcohol.Rare-earth ion solution, chlorine
Change aluminum solutions or the interpolation of deionized water is controlled by fluid flowmeter.Step（3）In, the barred body part containing weaker zone exists
Total time is soaked for 4-12 hour in solution.Step（4）In, when calculating the length that barred body soaks in the solution, need to consider
Due to adding the level change that solution or deionized water lead to.
With reference to Fig. 1, if in specific implementation process, need to mix in porous core layer three kinds or more kinds of rare earth from
Son, can add the devices such as corresponding cone-shaped glass container, solution conveyor tube road and fluid flowmeter in the entire system.With
Reason, if in specific implementation process, needs to mix three kinds in porous core layer or more kinds of is co-doped with ion, equally whole
The devices such as corresponding cone-shaped glass container, solution conveyor tube road and fluid flowmeter can be added in system.
Embodiment 1：The present embodiment is applied to making and has the preform that different ions are co-doped with ratio in the axial direction.For
Readily appreciate, the present embodiment taking the manufacturing process of relatively conventional erbium-ytterbium co-doped fiber prefabricated rods as a example illustrates.Profit first
Contain the prefabricated rods of porous core layer with MCVD process deposits, after the completion of deposition, take off the prefabricated rods 4 being connected to support tube 5, by folder
Tool 7 is fixed on automatically controlled precise elevating gear 6.In the first cone-shaped glass container 8, the second cone-shaped glass container 9, triconic glass
Be injected separately in glass container 10 and the 4th cone-shaped glass container 11 ytterbium ion solution, erbium ion solution, aluminium ion solution and go from
Sub- water, then opens first switch 12, second switch the 13, the 3rd switch 14 and the 4th switch 15, opening by controlling switch
Time, control first flowmeter 17, second flowmeter 18, the 3rd effusion meter 19 and the 4th effusion meter 20, four effusion meters are respectively
It is connected with four cone-shaped glass containers by solution conveyor tube road 16.Injection sets the ytterbium ion solution of volume, erbium in the container 1
Solion, aluminium ion solution and deionized water, then, are immersed prefabricated rods 4 in solution 2 by automatically controlled precise elevating gear.
Electric precision lowering or hoisting gear 6 is by computer program control.For improving prefabricated rods 4 utilization rate, automatically controlled precise elevating gear 6 is controlled to make
The interface position of prefabricated rods 4 and support tube 5 is maintained an equal level with liquid level 3.After abundant soak time t of prefabricated rods 4 (general t >=2 hour), will
Prefabricated rods 4 are lifted out solution 2, then, by controlling the opening time of second switch the 13, the 3rd switch 14 and the 4th switch 15
And, control second flowmeter 18, the 3rd effusion meter 19 and the 4th effusion meter 20, injection in the container 1 sets the erbium ion of volume
Solution, aluminium ion solution and deionized water, after solution mix homogeneously, a part of prefabricated rods 4 are immersed solution 2 again, stay
Prefabricated rods 4 length of liquid level 3 top is L/n, and wherein L represents the length of prefabricated rods, and n is to soak total degree.After soak time t,
Again prefabricated rods are lifted out solution 2, then again by controlling second switch the 13, the 3rd switch 14 and the 4th switch 15 beat
ETAD expected time of arrival and departure, controls second flowmeter 18, the 3rd effusion meter 19 and the 4th effusion meter 20, and injection in the container 1 sets the erbium of volume
A part of prefabricated rods 4, after solution mix homogeneously, are immersed solution by solion, aluminium ion solution and deionized water again, this
The length of the secondary prefabricated rods staying liquid level 3 top is 2L/n.Then, constantly repeat above procedure, so that during last immersion,
The prefabricated rods length of liquid level 3 lower section is L/n.Barred body part containing weaker zone soaks total time in the solution for 10 hours.?
The prefabricated rods 4 that total immersion is steeped after n time at last access MCVD lathe again.After drying and dehydrating, by weaker zone vitrification, finally will be hollow
Barred body collapsing becomes solid bar.According to embodiments above, just can prepare and on axial location, there are different ions and be co-doped with ratio
Erbium-ytterbium co-doped fiber prefabricated rods.
The manufacturing process that other has the rare earth ion co-doped fiber prefabricated rods that different ions are co-doped with ratio in the axial direction can
With reference to embodiment 1.
Embodiment 2：The present embodiment is applied to make and has same ion in the axial direction and be co-doped with ratio, different levels of doping
Preform.Contain the prefabricated rods of porous core layer first with MCVD process deposits, take off after the completion of deposition and be connected to support tube 5
Prefabricated rods 4, be fixed on automatically controlled precise elevating gear 6 by fixture 7.In the first cone-shaped glass container 8, the second cone-shaped glass
It is injected separately into A kind rare-earth ion solution, B kind rare earth in container 9, triconic glass container 10 and the 4th cone-shaped glass container 11
Solion, it is co-doped with solion and deionized water, then open first switch 12, second switch 13, the 3rd switch 14 and the
Four switches 15, by the opening time of controlling switch, control first flowmeter 17, second flowmeter 18, the 3rd effusion meter 19 and
4th effusion meter 20, four effusion meters are connected with four cone-shaped glass containers by solution conveyor tube road 16 respectively.In the container 1
Injection sets the A kind rare-earth ion solution of volume, B kind rare-earth ion solution, is co-doped with solion and deionized water, then, leads to
Cross automatically controlled precise elevating gear 6 by prefabricated 4 rod immersion solution 2, electric precision lowering or hoisting gear 6 is by computer program control.For
Improve prefabricated rods 4 utilization rate, control automatically controlled precise elevating gear so that prefabricated rods 4 and the interface position of support tube 5 is held with liquid level 3
Flat.After abundant soak time t of prefabricated rods 4 (general t >=2 hour), prefabricated rods 4 are lifted out solution 2, then, by controlling the
The opening time of four switches 15, controls the 4th effusion meter 20.Injection sets the deionized water of volume in the container 1, treats that solution mixes
After closing uniformly, a part of prefabricated rods 4 are immersed again solution 2, prefabricated rods 4 length staying liquid level 3 top is L/n.During immersion
Between after t, again prefabricated rods 4 are lifted out solution 2, then again by the opening time controlling the 4th switch 15, control the 4th
Effusion meter 20.Injection sets the deionized water of volume in the container 1, after solution mix homogeneously, again by a part of prefabricated rods 4
Immersion solution 2, the length that this stays the prefabricated rods of liquid level 3 top is 2L/n.Then, constantly repeat above procedure.Containing thin
The barred body part of loose layer soaks total time in the solution for 9 hours.The prefabricated rods 4 that total immersion is steeped after n time the most at last access again
MCVD lathe, after drying and dehydrating, hollow barred body collapsing is finally become solid bar by weaker zone vitrification.
Embodiment 3：The present embodiment is applied to making grade doping rare earth doped fiber prefabricated rods.First with MCVD process deposits
Prefabricated rods containing porous core layer, take off the prefabricated rods 4 being connected to support tube 5, are fixed on automatically controlled essence by fixture 7 after the completion of deposition
On close lowering or hoisting gear 6.In the first cone-shaped glass container 8, the second cone-shaped glass container 9, triconic glass container 10 and the 4th
It is injected separately into A kind rare-earth ion solution, B kind rare-earth ion solution in cone-shaped glass container 11, be co-doped with solion and deionization
Water, then open first switch 12, second switch the 13, the 3rd switch 14 and the 4th switch 15, by controlling switch when opening
Between, control first flowmeter 17, second flowmeter 18, the 3rd effusion meter 19 and the 4th effusion meter 20, four effusion meters lead to respectively
Cross solution conveyor tube road 16 to be connected with four cone-shaped glass containers.The A kind rare earth ion of injection setting volume is molten in the container 1
Liquid, B kind rare-earth ion solution, it is co-doped with solion and deionized water, then, by automatically controlled precise elevating gear 6 by prefabricated rods 4
In immersion solution 2, electric precision lowering or hoisting gear 6 is by computer program control.Abundant soak time t of prefabricated rods 41(general t >=2
Hour) after, start slowly to raise the height of prefabricated rods 4 using electric precision lowering or hoisting gear 6, meanwhile, open the 4th switch
15 and the 4th effusion meter 20, persistently injection sets the deionized water of flow in the container 1, finally, when prefabricated rods 4 exceed liquid completely
Behind face, close the 4th switch 15.The time t in this stage general2More than 8 hours.Barred body part containing weaker zone is in the solution
Soak total time for 10.5 hours.Prefabricated rods access MCVD lathe again the most at last, after drying and dehydrating, by weaker zone vitrification,
Finally hollow barred body collapsing is become solid bar.According to embodiments above, grade doping preform just can be prepared.
In sum, the invention provides a kind of core that effectively can make ion co-doped fiber prefabricated rods in the axial direction
There is the preparation method that different ions are co-doped with ratio and doping content.Cross-sectional structure using the prefabricated rods 4 of this method preparation
It is followed successively by quartz reaction tube wall 21, sealing coat 22, porous core layer 23 and hollow space 24 from outside to inside, as shown in Figure 2.
Claims (3)
1. a kind of preparation method of rare earth ion co-doped fiber prefabricated rods is it is characterised in that rare earth ion co-doped fiber prefabricated rods
Preparation adopt improved chemical vapor deposition method（MCVD）With solution doping technique, the method includes following preparation process：
（1）. prepare multiple rare earth ions respectively and aluminium ion is co-doped with the aqueous solution of agent；
（2）. select hollow quartz base tube barred body and access MCVD lathe, after high temperature polishing, be sequentially depositing sealing coat and loose core
Layer；
（3）. the hollow quartz base tube barred body containing porous core layer is fixed on electrical-controlled lifting device, initial period is it is ensured that contain
The hollow quartz base tube barred body part having porous core layer is completely soaked in the solution；
（4）. ratio distribution and concentration distribution are co-doped with to ion according to the excellent mandrel being pre-designed, change various ions in solution
It is co-doped with ratio and concentration, pass through electrical-controlled lifting device simultaneously and adjust the length that hollow quartz base tube barred body soaks in the solution；
（5）. soaked hollow quartz base tube barred body is accessed MCVD lathe again, after drying and dehydrating, by porous core layer glass
Change, finally hollow quartz base tube barred body collapsing is become solid bar.
2. a kind of preparation method of rare earth ion co-doped fiber prefabricated rods according to claim 1 is it is characterised in that described
Step（1）In, the aqueous solution that rare earth ion, aluminium ion are co-doped with agent adopts rare earth chloride, aluminum chloride and alcohol.
3. a kind of preparation method of rare earth ion co-doped fiber prefabricated rods according to claim 1 is it is characterised in that described
Step（3）And step（4）In, the hollow quartz base tube barred body part containing porous core layer soaks total time in the solution for 4-12
Hour.
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| CN110028236B (en) * | 2019-04-22 | 2020-08-18 | 华中科技大学 | Optical fiber with ion doping concentration gradually changing longitudinally and preparation method thereof |
| CN111574046A (en) * | 2020-05-29 | 2020-08-25 | 中国电子科技集团公司第四十六研究所 | Gas-liquid phase composite doping method for preparing rare earth doped optical fiber |
| CN111847864A (en) * | 2020-06-16 | 2020-10-30 | 武汉长进激光技术有限公司 | C-band expanded broadband gain erbium-doped optical fiber and preparation method thereof |
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| CN114199517A (en) * | 2021-12-10 | 2022-03-18 | 中国电子科技集团公司第四十六研究所 | Device and method for testing axial absorption uniformity of rare earth-doped optical fiber preform |
| CN217479333U (en) * | 2022-03-09 | 2022-09-23 | 华为技术有限公司 | Apparatus for doping a substrate tube comprising a porous layer |
| CN114721087B (en) * | 2022-06-08 | 2022-10-25 | 武汉长进激光技术有限公司 | Three-clad erbium-ytterbium co-doped optical fiber and preparation method and application thereof |
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